2-(1,1,2,2,2-pentafluoroethoxy)aniline

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 27.2 g of crude 2-pentafluoroethoxy-nitrobenzene, 2.6 g of Raney-nickel catalyst and 250 ml of dioxane is agitated in a hydrogen atmosphere for 24 hours at a temperature of 20°-25° C. The hydrogen consumption is 6.54 liters. After filtering off the catalyst, the solution is evaporated to dryness, yielding 20.5 g of 2-pentafluoroethoxy-aniline in form of a yellowish oil. The hydrogen consumption After filtering off the catalyst the solution is evaporated to dryness

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 27.2 g of crude 2-pentafluoroethoxy-nitrobenzene, 2.6 g of Raney-nickel catalyst and 250 ml of dioxane is agitated in a hydrogen atmosphere for 24 hours at a temperature of 20°-25° C. The hydrogen consumption is 6.54 liters. After filtering off the catalyst, the solution is evaporated to dryness, yielding 20.5 g of 2-pentafluoroethoxy-aniline in form of a yellowish oil. The hydrogen consumption After filtering off the catalyst the solution is evaporated to dryness

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: While cooling at 0° C., 101.2 g of a 40% solution of sodium hydrogen sulfite are added dropwise to a solution of 6.4 g of copper sulfate in 276 ml of 36% hydrochloric acid and 72 ml of water. To the resultant solution is then made the simultaneous dropwise addition of 101.2 g of a 40% solution of sodium hydrogen sulfite and a diazonium salt solution which has been cooled to -10° C. and obtained by the dropwise addition, with cooling, of 28.8 g of sodium nitrite in 44 ml of water to a solution of 39 ml of water, 84 ml of 36% hydrochloric acid and 90.8 g of 2-pentafluoroethoxy-aniline. During this addition the temperature of the reaction mixture rises to 30° C., accompanied by the simultaneous evolution of gas. The reaction mixture is stirred for 18 hours, whereupon a brown oil precipitates. The organic phase is separated and the aqueous phase is extracted with methylene chloride. The organic phases are combined and evaporated to dryness, affording crude 2-pentafluoroethoxyphenylsulfonyl chloride in the form of a brown oil. obtained by the dropwise addition During this addition the temperature of the reaction mixture rises to 30° C. precipitates The organic phase is separated the aqueous phase is extracted with methylene chloride evaporated to dryness

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: While cooling at 0° C., 101.2 g of a 40% solution of sodium hydrogen sulfite are added dropwise to a solution of 6.4 g of copper sulfate in 276 ml of 36% hydrochloric acid and 72 ml of water. To the resultant solution is then made the simultaneous dropwise addition of 101.2 g of a 40% solution of sodium hydrogen sulfite and a diazonium salt solution which has been cooled to -10° C. and obtained by the dropwise addition, with cooling, of 28.8 g of sodium nitrite in 44 ml of water to a solution of 39 ml of water, 84 ml of 36% hydrochloric acid and 90.8 g of 2-pentafluoroethoxy-aniline. During this addition the temperature of the reaction mixture rises to 30° C., accompanied by the simultaneous evolution of gas. The reaction mixture is stirred for 18 hours, whereupon a brown oil precipitates. The organic phase is separated and the aqueous phase is extracted with methylene chloride. The organic phases are combined and evaporated to dryness, affording crude 2-pentafluoroethoxyphenylsulfonyl chloride in the form of a brown oil. obtained by the dropwise addition During this addition the temperature of the reaction mixture rises to 30° C. precipitates The organic phase is separated the aqueous phase is extracted with methylene chloride evaporated to dryness

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: While cooling at 0° C., 101.2 g of a 40% solution of sodium hydrogen sulfite are added dropwise to a solution of 6.4 g of copper sulfate in 276 ml of 36% hydrochloric acid and 72 ml of water. To the resultant solution is then made the simultaneous dropwise addition of 101.2 g of a 40% solution of sodium hydrogen sulfite and a diazonium salt solution which has been cooled to -10° C. and obtained by the dropwise addition, with cooling, of 28.8 g of sodium nitrite in 44 ml of water to a solution of 39 ml of water, 84 ml of 36% hydrochloric acid and 90.8 g of 2-pentafluoroethoxy-aniline. During this addition the temperature of the reaction mixture rises to 30° C., accompanied by the simultaneous evolution of gas. The reaction mixture is stirred for 18 hours, whereupon a brown oil precipitates. The organic phase is separated and the aqueous phase is extracted with methylene chloride. The organic phases are combined and evaporated to dryness, affording crude 2-pentafluoroethoxyphenylsulfonyl chloride in the form of a brown oil. obtained by the dropwise addition During this addition the temperature of the reaction mixture rises to 30° C. precipitates The organic phase is separated the aqueous phase is extracted with methylene chloride evaporated to dryness

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 27.2 g of crude 2-pentafluoroethoxy-nitrobenzene, 2.6 g of Raney-nickel catalyst and 250 ml of dioxane is agitated in a hydrogen atmosphere for 24 hours at a temperature of 20°-25° C. The hydrogen consumption is 6.54 liters. After filtering off the catalyst, the solution is evaporated to dryness, yielding 20.5 g of 2-pentafluoroethoxy-aniline in form of a yellowish oil. The hydrogen consumption After filtering off the catalyst the solution is evaporated to dryness

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: While cooling at 0° C., 101.2 g of a 40% solution of sodium hydrogen sulfite are added dropwise to a solution of 6.4 g of copper sulfate in 276 ml of 36% hydrochloric acid and 72 ml of water. To the resultant solution is then made the simultaneous dropwise addition of 101.2 g of a 40% solution of sodium hydrogen sulfite and a diazonium salt solution which has been cooled to -10° C. and obtained by the dropwise addition, with cooling, of 28.8 g of sodium nitrite in 44 ml of water to a solution of 39 ml of water, 84 ml of 36% hydrochloric acid and 90.8 g of 2-pentafluoroethoxy-aniline. During this addition the temperature of the reaction mixture rises to 30° C., accompanied by the simultaneous evolution of gas. The reaction mixture is stirred for 18 hours, whereupon a brown oil precipitates. The organic phase is separated and the aqueous phase is extracted with methylene chloride. The organic phases are combined and evaporated to dryness, affording crude 2-pentafluoroethoxyphenylsulfonyl chloride in the form of a brown oil. obtained by the dropwise addition During this addition the temperature of the reaction mixture rises to 30° C. precipitates The organic phase is separated the aqueous phase is extracted with methylene chloride evaporated to dryness